JP4536781B2 - Electroless nickel plating solution - Google Patents
Electroless nickel plating solution Download PDFInfo
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- JP4536781B2 JP4536781B2 JP2007539858A JP2007539858A JP4536781B2 JP 4536781 B2 JP4536781 B2 JP 4536781B2 JP 2007539858 A JP2007539858 A JP 2007539858A JP 2007539858 A JP2007539858 A JP 2007539858A JP 4536781 B2 JP4536781 B2 JP 4536781B2
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1675—Process conditions
- C23C18/1683—Control of electrolyte composition, e.g. measurement, adjustment
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/24—Reinforcing the conductive pattern
- H05K3/244—Finish plating of conductors, especially of copper conductors, e.g. for pads or lands
Description
本発明は、無電解ニッケルめっき液に関する。特に、多数のＩＣチップからなるシリコンウエハー上に無電解ＮｉめっきによるＮｉ金属バンプ（突起部）もしくははんだバンプ用のニッケルアンダーバリアメタル（ＵＢＭ）を均一な膜厚で形成することを可能とする無電解Ｎｉめっき液に関する。 The present invention relates to an electroless nickel plating solution. In particular, it is possible to form Ni metal bumps (protrusions) by electroless Ni plating or nickel under barrier metal (UBM) for solder bumps on a silicon wafer composed of a large number of IC chips with a uniform film thickness. The present invention relates to an electrolytic Ni plating solution.
無電解めっき法によるめっきは、材料表面の接触作用による還元を利用しているため、窪んだ所にも一様な厚さにめっきをすることができる。特に、一般的に無電解Ｎｉめっきは耐食性、耐磨耗性に優れているため、古くから材料部品の表面処理用めっきとして使用されておりその歴史は古い。近年ではプリント配線板のはんだ接合の下地処理用もしくはコンパクトディスク（ＣＤ）、ハードディスクドライブ（ＨＤＤ）の下地処理用として広く使用されている。 Since the plating by the electroless plating method uses reduction by the contact action of the material surface, it is possible to plate even a recessed portion with a uniform thickness. In particular, since electroless Ni plating is generally excellent in corrosion resistance and wear resistance, it has long been used as a plating for surface treatment of material parts and has a long history. In recent years, it has been widely used for ground processing of solder joints of printed wiring boards or for ground processing of compact discs (CD) and hard disk drives (HDD).
はんだの下地処理として広く一般的に使用されている無電解ニッケルめっき液には、安定剤として鉛化合物が含有されているため、得られるニッケル皮膜にも鉛が含有される。
しかし、最近ＥＵ（ヨーロッパ連合）のＲｏＨＳ法の制定により、電子部品中の鉛、クロム等の有害物質の規制が強化され（現在鉛は０．１％以下）、今後その規制はさらに厳しくなるものと考えられている。また、はんだの種類も以前はスズと鉛の共晶はんだが一般的であったが、最近は鉛フリーのスズ・銀・亜鉛もしくはスズ・銀・ビスマス等の２元系もしくは３元系のはんだが実用化されている。以上のようにＲｏＨＳ法の規制ははんだのみならず、電子部品全般に規制がかけられているために、はんだの下地処理として広く一般的に使用されている無電解法によるニッケル皮膜にもこの規制が適用される。例えば、ニッケル皮膜の耐食性及びはんだ濡れ性の低下を改善した特許文献１に記載された無電解ニッケルめっき法においてもＲｏＨＳ法の規制を考慮しなければならない。Since the electroless nickel plating solution widely used as a solder base treatment contains a lead compound as a stabilizer, the resulting nickel coating also contains lead.
However, recently the EU (European Union) RoHS regulation has strengthened regulations on harmful substances such as lead and chromium in electronic components (currently lead is less than 0.1%), and the regulations will become even stricter in the future. It is believed that. In addition, the eutectic solder of tin and lead was common before, but recently, lead-free tin / silver / zinc or tin / silver / bismuth etc. binary or ternary solder Has been put to practical use. As described above, the regulation of the RoHS method is not only applied to solder but also to electronic components in general, and this regulation is applied to the electroless nickel coating that is widely used as a base treatment for solder. Applies. For example, in the electroless nickel plating method described in Patent Document 1 in which the deterioration of the corrosion resistance and solder wettability of the nickel film is improved, the regulation of the RoHS method must be considered.
さらに多数のＩＣからなるシリコンウエハー上に無電解ニッケルめっきによりニッケル金属バンプ（突起部）もしくははんだバンプ用のニッケルアンダーバリアメタル（ＵＢＭ）を形成しようとした場合、集積回路内の電位差の問題（例えばｎ型半導体（Ｓｉ中に微量のリンをドーピングしたもの）にさらにボロンをドーピングしてｐ型半導体を作ると、接合面にｎ／ｐ拡散層ができ、１００ルクスの光をこのＩＣに当てるとＰ／Ｎ極間に約０．４Ｖの電位差が発生する。）、もしくは電極パッド（材質はアルミニウムもしくは銅が一般的）の微細化により、電極パッド上に析出させたニッケル金属の高さが不揃いとなったり、ひどい場合にはニッケル金属が全く析出しないという新たな問題がでてくる。このように複数の問題が依然として解決されていないため、無電解ニッケル液はシリコンウエハー用バンプもしくはＵＢＮとして使用することが困難であると考えられている。 Furthermore, when an attempt is made to form nickel metal bumps (protrusions) or nickel under barrier metal (UBM) for solder bumps on a silicon wafer consisting of a large number of ICs by electroless nickel plating, problems such as potential differences in the integrated circuit (for example, When a p-type semiconductor is made by further doping boron into an n-type semiconductor (which is doped with a small amount of phosphorus in Si), an n / p diffusion layer is formed on the junction surface, and 100 lux light is applied to this IC A potential difference of about 0.4 V is generated between the P / N poles), or the height of the nickel metal deposited on the electrode pad is uneven due to the miniaturization of the electrode pad (material is typically aluminum or copper). In the worst case, there is a new problem that nickel metal does not precipitate at all. As described above, since a plurality of problems have not been solved yet, it is considered that the electroless nickel solution is difficult to be used as a bump or UBN for a silicon wafer.
このため、現在は電気金（Ａｕ）めっき法により、高さがおよそ１５μｍのＡｕバンプが作製されたり、ＵＢＭ用にスパッタもしくは電気めっき法の併用により、高さがおよそ５μｍのバリアー金属が作製され利用されている。しかし、Ａｕめっき法は工程が複雑でかつコストが高く、またスパッタ及び電気めっき法では電気を供給するシード層及び拡散防止層をエッチングしなければならず工程が複雑になり生産性を下げている。
本発明は、無電解ニッケルめっきにより半導体ウエハー上にニッケル金属バンプもしくははんだバンプ用のＵＢＭを形成しても、電極パッド上に析出されたニッケル金属の高さが不揃いとならずに、均一な厚さとなり、かつＲｏＨＳ法の規制を満足する鉛含有量の少ない無電解ニッケルめっき液を提供することを目的とする。 In the present invention, even when a nickel metal bump or a solder bump UBM is formed on a semiconductor wafer by electroless nickel plating, the height of the nickel metal deposited on the electrode pad is not uneven, and the thickness is uniform. An object of the present invention is to provide an electroless nickel plating solution with a low lead content that satisfies the regulations of the RoHS method.
上記課題を解決するために鋭意検討を重ねた結果、無電解ニッケルめっき液に特定の濃度の鉛イオン、コバルトイオン及びイオウ化合物を含有させることが有効であることを知見し、本発明に至った。
すなわち本発明は、
水溶性ニッケル塩、還元剤、錯化剤、ｐＨ緩衝剤を含有する無電解ニッケルめっき液において、鉛イオンを０．０１〜１ｐｐｍ、コバルトイオンを０．０１〜１ｐｐｍ、及びイオウ化合物を０．０１〜１ｐｐｍ含有する無電解ニッケルめっき液に関する。As a result of intensive studies to solve the above problems, it has been found that it is effective to contain lead ions, cobalt ions and sulfur compounds at specific concentrations in the electroless nickel plating solution, and the present invention has been achieved. .
That is, the present invention
In an electroless nickel plating solution containing a water-soluble nickel salt, a reducing agent, a complexing agent, and a pH buffer, lead ions are 0.01 to 1 ppm, cobalt ions are 0.01 to 1 ppm, and sulfur compounds are 0.01. It relates to an electroless nickel plating solution containing ˜1 ppm.
本発明の無電解ニッケルめっき液を使用することにより、ＲｏＨＳ法を満足し、かつ多数のＩＣチップからなるシリコンウエハー上に無電解ＮｉめっきによるＮｉ金属バンプもしくははんだバンプ用のＵＢＭを均一な膜厚で形成することができる。これにより、コストが高く複雑な工程を経るＡｕめっき法やスパッタ及び電気めっき法を利用することなく、安価で簡便に金属バンプ、ＵＢＭを作製することが可能となる。 By using the electroless nickel plating solution of the present invention, a UHS for Ni metal bumps or solder bumps by electroless Ni plating is uniformly formed on a silicon wafer consisting of a large number of IC chips that satisfies the RoHS method. Can be formed. This makes it possible to easily and inexpensively produce metal bumps and UBMs without using an Au plating method, sputtering, and electroplating method that are expensive and complicated.
本発明の無電解ニッケルめっき液は、水溶性ニッケル塩、還元剤、ｐＨ緩衝剤、錯化剤を含有し、更に所定濃度の鉛イオン、コバルトイオン、及びイオウ化合物を含有するが、その他必要に応じて安定剤、反応促進剤、界面活性剤などを含有することができる。 The electroless nickel plating solution of the present invention contains a water-soluble nickel salt, a reducing agent, a pH buffering agent, a complexing agent, and further contains lead ions, cobalt ions, and a sulfur compound at a predetermined concentration, but other necessity. Accordingly, stabilizers, reaction accelerators, surfactants and the like can be contained.
本発明の無電解ニッケルめっき液において使用する水溶性ニッケル塩としては、例えば硫酸ニッケル、塩化ニッケル、次亜リン酸ニッケル、などがあげられる。
還元剤としては、例えば、次亜リン酸塩、ジメチルアミンボラン、トリメチルアミンボラン、ヒドラジンなどが挙げられる。
ｐＨ緩衝剤としては、例えば酢酸、蟻酸、コハク酸、マロン酸等のカルボン酸塩、アンモニウム塩等が挙げられる。Examples of the water-soluble nickel salt used in the electroless nickel plating solution of the present invention include nickel sulfate, nickel chloride, nickel hypophosphite, and the like.
Examples of the reducing agent include hypophosphite, dimethylamine borane, trimethylamine borane, hydrazine and the like.
Examples of the pH buffer include carboxylic acid salts such as acetic acid, formic acid, succinic acid, and malonic acid, ammonium salts, and the like.
錯化剤としては、例えば乳酸、りんご酸、クエン酸等のオキシカルボン酸、グリシン、アラニン等のアミノ酸類等が挙げられる。
本発明においては、鉛イオン、イオウ化合物は安定剤となるが、さらに安定剤として、その他の安定剤を含有しても良く、例えば、ビスマス、セレン、タリウム等の重金属イオン等が挙げられる。Examples of the complexing agent include oxycarboxylic acids such as lactic acid, malic acid and citric acid, and amino acids such as glycine and alanine.
In the present invention, lead ions and sulfur compounds serve as stabilizers, but may further contain other stabilizers as stabilizers, for example, heavy metal ions such as bismuth, selenium and thallium.
反応促進剤としては、例えばエチレンジアミン、トリエチレンテトラミン等のアミン系化合物等が挙げられる。
界面活性剤としては、例えばポリエチレングリコール等の非イオン系アルコール、スルホン酸系の陰イオン系界面活性剤、アミンオキサイド系の陽イオン系界面活性剤等が挙げられる。Examples of the reaction accelerator include amine compounds such as ethylenediamine and triethylenetetramine.
Examples of the surfactant include nonionic alcohols such as polyethylene glycol, sulfonic acid anionic surfactants, and amine oxide cationic surfactants.
ＲｏＨＳ法のニッケル皮膜中に含有される鉛の濃度の問題を克服するためには無電解ニッケルめっき液中の鉛イオンの濃度を低下させることは必要不可欠な条件であるが、単純に鉛イオンの濃度を低下させるとニッケル電着面の四隅にニッケルのこぶ状の異常電着が発生するので、このこぶ状の異常電着を抑制するために必要最低限の鉛イオンの濃度が無電解ニッケルめっき液に必要である。このこぶ状の異常電着は、イオウ系化合物の濃度が高いと抑制することができるが、微細電極パッドにＮｉが析出しなくなる。 In order to overcome the problem of the concentration of lead contained in the nickel film of the RoHS method, it is indispensable to reduce the concentration of lead ions in the electroless nickel plating solution. If the concentration is lowered, abnormal nickel electrodeposition occurs at the four corners of the nickel electrodeposition surface. The minimum lead ion concentration necessary to suppress this abnormal electrodeposition is not electroless nickel plating. Necessary for the liquid. This bumpy abnormal electrodeposition can be suppressed when the concentration of the sulfur compound is high, but Ni does not precipitate on the fine electrode pad.
また、本発明に係る、半導体固有の電位差の問題を克服し、かつ微細電極パッド上にバンプを形成することのできる無電解Ｎｉめっき液を作製するのに重要な点は、コバルトイオンの添加とイオウ化合物の添加の両方が必要不可決な点である。この２種類の添加物のどちらか一方が欠如すると、半導体固有の電位差を有する電極パッド上に析出するＮｉの厚さにばらつきが生じ、酷い場合にはどちらか一方の電極にＮｉが析出しなかったりする。また微細化された電極パッド上にも同様にＮｉが析出しなかったり、厚みに大きなばらつきが発生したりする。
よって、無電解ニッケル液中の鉛イオン、コバルトイオン及びイオウ化合物の３つは相互に影響するのでこの３成分の適正濃度を把握することが重要である。In addition, the important point for producing the electroless Ni plating solution that can overcome the problem of potential difference inherent to the semiconductor and can form bumps on the fine electrode pad according to the present invention is the addition of cobalt ions. Both additions of sulfur compounds are necessary and inevitable. If either one of these two types of additives is absent, the Ni thickness deposited on the electrode pad having the potential difference inherent to the semiconductor will vary, and in severe cases, Ni will not deposit on either electrode. Or Similarly, Ni does not precipitate on the miniaturized electrode pad, or the thickness varies greatly.
Therefore, since the three of lead ion, cobalt ion and sulfur compound in the electroless nickel solution affect each other, it is important to grasp the proper concentration of these three components.
本発明の無電解ニッケルめっき液においては、鉛イオンを０．０１〜１ｐｐｍ含有することが重要である。より好ましくは０．１ｐｐｍ〜１ｐｐｍである。０．０１ｐｐｍ未満の場合、ニッケル電着面の四隅にニッケルのこぶ状の異常電着が発生しやすい。この異常電着の発生は鉛イオンが前記の範囲内にあれば、抑制することができる。１ｐｐｍを越える場合、ニッケル皮膜中の鉛の含有量がおよそ３００ｐｐｍを超えることになる。ＲｏＨＳ法では１０００ｐｐｍ（０．１％）以下を要求されているが、将来を見据え、その他必要特性を満たすのであれば、より低濃度化するのが望ましい。１ｐｐｍを越えて添加しても、ニッケル中の鉛の含有量が増加するのみである。
めっき液中に鉛イオンを含有させるためには、鉛化合物をめっき液に溶解すればよく、該鉛化合物としては、硝酸鉛、酢酸鉛等を挙げることができる。In the electroless nickel plating solution of the present invention, it is important to contain 0.01 to 1 ppm of lead ions. More preferably, it is 0.1 ppm to 1 ppm. When the concentration is less than 0.01 ppm, nickel bumpy abnormal electrodeposition tends to occur at the four corners of the nickel electrodeposition surface. Generation | occurrence | production of this abnormal electrodeposition can be suppressed if lead ion exists in the said range. When it exceeds 1 ppm, the lead content in the nickel film exceeds approximately 300 ppm. In the RoHS method, 1000 ppm (0.1%) or less is required, but it is desirable to lower the concentration if other necessary characteristics are satisfied with the future in mind. Adding over 1 ppm only increases the lead content in the nickel.
In order to contain lead ions in the plating solution, a lead compound may be dissolved in the plating solution, and examples of the lead compound include lead nitrate and lead acetate.
また、コバルトイオンを０．０１ｐｐｍ〜１ｐｐｍ含有していることが重要である。より好ましくは、０．３ｐｐｍ〜１ｐｐｍである。コバルト無添加の場合はイオウ化合物を添加してもニッケルの析出速度が遅くなり、かつ電位差の影響を受け、特に半導体電極のＮ極にニッケルが析出しなくなる。本発明の所期の目的を達成するためにはコバルトイオンを０．０１ｐｐｍ以上めっき液中に含有させる必要があるが、１ｐｐｍを越える高濃度にすると、添加初期、ニッケル表面にピンホールが発生し易くなってしまう。ニッケル表面のピンホールは無電解置換金めっき時、孔食の原因になるので、はんだ接合強度の点から好ましくない。
めっき液中にコバルトイオンを含有させるには、コバルト化合物をめっき液中に溶解すればよく、該コバルト化合物としては、硫酸コバルト、酢酸コバルト、硝酸コバルト、炭酸コバルト等を挙げることができる。Moreover, it is important to contain 0.01 ppm to 1 ppm of cobalt ions. More preferably, it is 0.3 ppm to 1 ppm. In the case of no addition of cobalt, even if a sulfur compound is added, the deposition rate of nickel becomes slow and is affected by the potential difference, so that nickel does not precipitate particularly at the N pole of the semiconductor electrode. In order to achieve the intended object of the present invention, cobalt ions must be contained in the plating solution in an amount of 0.01 ppm or more. However, if the concentration exceeds 1 ppm, pinholes are generated on the nickel surface in the initial stage of addition. It becomes easy. Since pinholes on the nickel surface cause pitting corrosion during electroless substitution gold plating, it is not preferable from the viewpoint of solder joint strength.
In order to contain cobalt ions in the plating solution, a cobalt compound may be dissolved in the plating solution, and examples of the cobalt compound include cobalt sulfate, cobalt acetate, cobalt nitrate, and cobalt carbonate.
次にイオウ化合物の無電解ニッケルめっき液中の濃度についても重要であり、０．０１〜１ｐｐｍ含有する必要がある。より好ましくは、０．１〜０．５ｐｐｍである。イオウ化合物はコバルト同様にこれを無添加とした場合はニッケルの析出速度が遅くなり、かつ電位差の影響を受け、特に半導体電極のＮ極にニッケルが析出しなくなる。本発明の所期の目的を達成するためにはイオウ化合物の濃度は０．０１ｐｐｍ以上必要である。イオウ化合物の濃度が１ｐｐｍを越えて含有している場合には、微細パッド部にニッケルが析出し難くなる。
本発明に使用するイオウ化合物は、チオ硫酸塩、チオン酸塩、チオ尿素、チオシアン酸塩、チオ炭酸塩、あるいはこれらの塩等が好ましい。特に好ましいのは、チオシアン酸カリウム（別名、ロダンカリ）、ロダニンである。Next, it is important also about the density | concentration in the electroless nickel plating solution of a sulfur compound, and it is necessary to contain 0.01-1 ppm. More preferably, it is 0.1-0.5 ppm. If the sulfur compound is not added like cobalt, the deposition rate of nickel is slow, and it is affected by the potential difference, and nickel is not particularly deposited at the N pole of the semiconductor electrode. In order to achieve the intended object of the present invention, the concentration of the sulfur compound needs to be 0.01 ppm or more. When the concentration of the sulfur compound exceeds 1 ppm, nickel hardly deposits on the fine pad portion.
The sulfur compound used in the present invention is preferably thiosulfate, thionate, thiourea, thiocyanate, thiocarbonate, or a salt thereof. Particularly preferred are potassium thiocyanate (also known as rodankari) and rhodanine.
本発明の無電解ニッケルめっき液は、水溶液であり、ｐＨ４〜６に調整することが好ましく、ｐＨ４．５〜５．５に調整することがより好ましい。
また、本発明の無電解ニッケルめっき液は、浴温７０〜９０℃で使用するのが好ましく、７５〜８５℃がより好ましい。
めっき液のｐＨ、及び浴温が上記範囲外の場合、めっき速度が遅かったり、浴分解を起し易い等の問題がある。
めっき方法としては、本発明のめっき液中に被めっき物を浸漬すればよい。The electroless nickel plating solution of the present invention is an aqueous solution, preferably adjusted to pH 4 to 6, and more preferably adjusted to pH 4.5 to 5.5.
Further, the electroless nickel plating solution of the present invention is preferably used at a bath temperature of 70 to 90 ° C, more preferably 75 to 85 ° C.
When the pH of the plating solution and the bath temperature are out of the above ranges, there are problems such as a slow plating rate and easy decomposition of the bath.
What is necessary is just to immerse a to-be-plated object in the plating solution of this invention as a plating method.
以下、本発明を実施例に基づいて説明するが、本発明はこれに限定されるものではない。
［実施例１］
以下の組成の無電解ニッケルめっき液を建浴した。
ＮｉＳＯ４・６Ｈ２Ｏ ２５ｇ／ｌ
ＮａＨ２ＰＯ２・Ｈ２Ｏ ２５ｇ／ｌ
りんご酸 ４ｇ／ｌ
コハク酸２Ｎａ １２ｇ／ｌ
グリシン ５ｇ／ｌ
Ｐｂ（ＮＯ３）２ ０．６ｐｐｍ（Ｐｂとして０．３８ｐｐｍ）
ＣｏＳＯ４・７Ｈ２Ｏ １．６ｐｐｍ（Ｃｏとして０．３２ｐｐｍ）
ＫＳＣＮ ０．４ｐｐｍ
該無電解ニッケルめっき液を用いて無電解ニッケルめっきを施した。なお、ｐＨは５．０とし、めっき条件は８０℃で３０分とした。被めっき材は多数のＩＣからなる半導体ＴＥＧウエハー（ｎ／ｐ電極有り）であり、約１００ルックスの自然光下の条件のもとにこのＩＣのアルミニウムパッド上にニッケルを析出させた。EXAMPLES Hereinafter, although this invention is demonstrated based on an Example, this invention is not limited to this.
[Example 1]
An electroless nickel plating solution having the following composition was constructed.
NiSO 4 · 6H 2 O 25g / l
NaH 2 PO 2 · H 2 O 25g / l
Malic acid 4g / l
Succinic acid 2Na 12g / l
Glycine 5g / l
Pb (NO 3 ) 2 0.6 ppm (0.38 ppm as Pb)
CoSO 4 · 7H 2 O 1.6 ppm (0.32 ppm as Co)
KSCN 0.4ppm
Electroless nickel plating was performed using the electroless nickel plating solution. The pH was 5.0 and the plating conditions were 80 ° C. and 30 minutes. The material to be plated was a semiconductor TEG wafer (with n / p electrodes) consisting of a large number of ICs, and nickel was deposited on the aluminum pads of the ICs under conditions of about 100 lux under natural light.
［比較例１］
以下の組成の無電解ニッケルめっき液を建浴した。
ＮｉＳＯ４・６Ｈ２Ｏ ２５ｇ／ｌ
ＮａＨ２ＰＯ２・Ｈ２Ｏ ２５ｇ／ｌ
りんご酸 ４ｇ／ｌ
コハク酸２Ｎａ １２ｇ／ｌ
グリシン ５ｇ／ｌ
Ｐｂ（ＮＯ３）２ ０．６ｐｐｍ（Ｐｂとして０．３８ｐｐｍ）
ＣｏＳＯ４・７Ｈ２Ｏ １６ｐｐｍ（Ｃｏとして３．２ｐｐｍ）
ＫＳＣＮ ０．４ｐｐｍ
該無電解ニッケルめっき液を用いて無電解ニッケルめっきを施した。なお、ｐＨは５．０とし、めっき条件は８０℃で３０分とした。被めっき材は多数のＩＣからなる半導体ＴＥＧウエハー（ｎ／ｐ電極有り）であり、約１００ルクスの自然光下の条件の下にこのＩＣのアルミニウムパッド上にニッケルを析出させた。[Comparative Example 1]
An electroless nickel plating solution having the following composition was constructed.
NiSO 4 · 6H 2 O 25g / l
NaH 2 PO 2 · H 2 O 25g / l
Malic acid 4g / l
Succinic acid 2Na 12g / l
Glycine 5g / l
Pb (NO 3 ) 2 0.6 ppm (0.38 ppm as Pb)
CoSO 4 · 7H 2 O 16ppm ( 3.2ppm as Co)
KSCN 0.4ppm
Electroless nickel plating was performed using the electroless nickel plating solution. The pH was 5.0 and the plating conditions were 80 ° C. and 30 minutes. The material to be plated was a semiconductor TEG wafer (with n / p electrodes) consisting of a large number of ICs, and nickel was deposited on the aluminum pads of the ICs under conditions of about 100 lux under natural light.
［比較例２］
以下の組成の無電解ニッケルめっき液を建浴した。
ＮｉＳＯ４・６Ｈ２Ｏ ２５ｇ／ｌ
ＮａＨ２ＰＯ２・Ｈ２Ｏ ２５ｇ／ｌ
りんご酸 ４ｇ／ｌ
コハク酸２Ｎａ １２ｇ／ｌ
グリシン ５ｇ／ｌ
Ｐｂ（ＮＯ３）２ ０．６ｐｐｍ（Ｐｂとして０．３８ｐｐｍ）
ＣｏＳＯ４・７Ｈ２Ｏ １６０ｐｐｍ（Ｃｏとして３２ｐｐｍ）
ＫＳＣＮ ０．４ｐｐｍ
該無電解ニッケルめっき液を用いて無電解ニッケルめっきを施した。なお、ｐＨは５．０とし、めっき条件は８０℃で３０分とした。被めっき材は多数のＩＣからなる半導体ＴＥＧウエハー（ｎ／ｐ電極有り）であり、約１００ルクスの自然光下の条件の下にこのＩＣのアルミニウムパッド上にニッケルを析出させた。[Comparative Example 2]
An electroless nickel plating solution having the following composition was constructed.
NiSO 4 · 6H 2 O 25g / l
NaH 2 PO 2 · H 2 O 25g / l
Malic acid 4g / l
Succinic acid 2Na 12g / l
Glycine 5g / l
Pb (NO 3 ) 2 0.6 ppm (0.38 ppm as Pb)
CoSO 4 · 7H 2 O 160ppm ( 32ppm as Co)
KSCN 0.4ppm
Electroless nickel plating was performed using the electroless nickel plating solution. The pH was 5.0 and the plating conditions were 80 ° C. and 30 minutes. The material to be plated was a semiconductor TEG wafer (with n / p electrodes) consisting of a large number of ICs, and nickel was deposited on the aluminum pads of the ICs under conditions of about 100 lux under natural light.
［比較例３］
以下の組成の無電解ニッケルめっき液を建浴した。
ＮｉＳＯ４・６Ｈ２Ｏ ２５ｇ／ｌ
ＮａＨ２ＰＯ２・Ｈ２Ｏ ２５ｇ／ｌ
りんご酸 ４ｇ／ｌ
コハク酸２Ｎａ １２ｇ／ｌ
グリシン ５ｇ／ｌ
Ｐｂ（ＮＯ３）２ ０．６ｐｐｍ（Ｐｂとして０．３８ｐｐｍ）
ＣｏＳＯ４・７Ｈ２Ｏ ０ｐｐｍ
ＫＳＣＮ ０．４ｐｐｍ
該無電解ニッケルめっき液を用いて無電解ニッケルめっきを施した。なお、ｐＨは５．０とし、めっき条件は８０℃で３０分とした。被めっき材は多数のＩＣからなる半導体ＴＥＧウエハー（ｎ／ｐ電極有り）であり、約１００ルクスの自然光下の条件のもとにこのＩＣのアルミニウムパッド上にニッケルを析出させた。[Comparative Example 3]
An electroless nickel plating solution having the following composition was constructed.
NiSO 4 · 6H 2 O 25g / l
NaH 2 PO 2 · H 2 O 25g / l
Malic acid 4g / l
Succinic acid 2Na 12g / l
Glycine 5g / l
Pb (NO 3 ) 2 0.6 ppm (0.38 ppm as Pb)
CoSO 4 · 7H 2 O 0ppm
KSCN 0.4ppm
Electroless nickel plating was performed using the electroless nickel plating solution. The pH was 5.0 and the plating conditions were 80 ° C. and 30 minutes. The material to be plated was a semiconductor TEG wafer (with n / p electrodes) consisting of a large number of ICs, and nickel was deposited on the aluminum pads of the ICs under conditions of about 100 lux under natural light.
［比較例４］
以下の組成の無電解ニッケルめっき液を建浴した。
ＮｉＳＯ４・６Ｈ２Ｏ ２５ｇ／ｌ
ＮａＨ２ＰＯ２・Ｈ２Ｏ ２５ｇ／ｌ
りんご酸 ４ｇ／ｌ
コハク酸２Ｎａ １２ｇ／ｌ
グリシン ５ｇ／ｌ
Ｐｂ（ＮＯ３）２ ０ｐｐｍ
ＣｏＳＯ４・７Ｈ２Ｏ １６ｐｐｍ（Ｃｏとして３．２ｐｐｍ）
ＫＳＣＮ ０．４ｐｐｍ
該無電解ニッケルめっき液を用いて無電解ニッケルめっきを施した。なお、ｐＨは５．０とし、めっき条件は８０℃で３０分とした。被めっき材は多数のＩＣからなる半導体ＴＥＧウエハー（ｎ／ｐ電極有り）であり、約１００ルクスの自然光下の条件のもとにこのＩＣのアルミニウムパッド上にニッケルを析出させた。[Comparative Example 4]
An electroless nickel plating solution having the following composition was constructed.
NiSO 4 · 6H 2 O 25g / l
NaH 2 PO 2 · H 2 O 25g / l
Malic acid 4g / l
Succinic acid 2Na 12g / l
Glycine 5g / l
Pb (NO 3 ) 20 ppm
CoSO 4 · 7H 2 O 16ppm ( 3.2ppm as Co)
KSCN 0.4ppm
Electroless nickel plating was performed using the electroless nickel plating solution. The pH was 5.0 and the plating conditions were 80 ° C. and 30 minutes. The material to be plated was a semiconductor TEG wafer (with n / p electrodes) consisting of a large number of ICs, and nickel was deposited on the aluminum pads of the ICs under conditions of about 100 lux under natural light.
［比較例５］
以下の組成の無電解ニッケルめっき液を建浴した。
ＮｉＳＯ４・６Ｈ２Ｏ ２５ｇ／ｌ
ＮａＨ２ＰＯ２・Ｈ２Ｏ ２５ｇ／ｌ
りんご酸 ４ｇ／ｌ
コハク酸２Ｎａ １２ｇ／ｌ
グリシン ５ｇ／ｌ
Ｐｂ（ＮＯ３）２ ０．６ｐｐｍ
ＣｏＳＯ４・７Ｈ２Ｏ １６ｐｐｍ（Ｃｏとして３．２ｐｐｍ）
該無電解ニッケルめっき液を用いて無電解ニッケルめっきを施した。なお、ｐＨは５．０とし、めっき条件は８０℃で３０分とした。被めっき材は多数のＩＣからなる半導体ＴＥＧウエハー（ｎ／ｐ電極有り）であり、約１００ルクスの自然光下の条件のもとにこのＩＣのアルミニウムパッド上にニッケルを析出させた。[Comparative Example 5]
An electroless nickel plating solution having the following composition was constructed.
NiSO 4 · 6H 2 O 25g / l
NaH 2 PO 2 · H 2 O 25g / l
Malic acid 4g / l
Succinic acid 2Na 12g / l
Glycine 5g / l
Pb (NO 3 ) 2 0.6 ppm
CoSO 4 · 7H 2 O 16ppm ( 3.2ppm as Co)
Electroless nickel plating was performed using the electroless nickel plating solution. The pH was 5.0 and the plating conditions were 80 ° C. and 30 minutes. The material to be plated was a semiconductor TEG wafer (with n / p electrodes) consisting of a large number of ICs, and nickel was deposited on the aluminum pads of the ICs under conditions of about 100 lux under natural light.
実施例により施された無電解Ｎｉめっきの顕微鏡及び電子顕微鏡による拡大写真を図１に示した。同様に比較例１〜５によるものをそれぞれ図２〜６に示した。更に実施例及び比較例１〜５によりＡｌパッド上に析出したニッケルを評価した結果の詳細を表にまとめた。なお、各評価項目とその評価方法は以下に示すとおりである。 An enlarged photograph of the electroless Ni plating applied according to the example using a microscope and an electron microscope is shown in FIG. Similarly, those according to Comparative Examples 1 to 5 are shown in FIGS. Further, details of the results of evaluation of nickel deposited on the Al pad in Examples and Comparative Examples 1 to 5 are summarized in a table. In addition, each evaluation item and its evaluation method are as showing below.
Ｎｉ高さＰ極およびＮ極：レーザー顕微鏡によりＰ極およびＮ極上のＮｉの高さを測定した。
Ｐ／Ｎ高さ比：上記測定後Ｐ／Ｎ高さ比を計算した。
ピンホール：ＳＥＭにより５０００倍に拡大し、ピンホールの有無を観察した。
異常析出（こぶ）：ＳＥＭにより５００倍に拡大し、異常析出（こぶ）を観察した。
Ｐｂ含有量：析出したニッケル中の含有量で、ＧＤＭＡＳ分析により測定した。Ni height P pole and N pole: The height of Ni on the P pole and the N pole was measured by a laser microscope.
P / N height ratio: After the above measurement, the P / N height ratio was calculated.
Pinhole: It was magnified 5000 times by SEM and the presence or absence of a pinhole was observed.
Abnormal precipitation (gump): Magnified by SEM by 500 times, and abnormal precipitation (gump) was observed.
Pb content: The content in precipitated nickel, which was measured by GDMAS analysis.
図１からも明らかなように本発明に係る無電解Ｎｉめっき液を使用した実施例においては、Ａｌパッド上にＩＣ固有の電位差及び面積の影響も受けず均一な無電解Ｎｉめっきを施すことができ、Ｎｉの析出速度も十分であり、かつ、比較例に見られるようなＮｉのピンホール及び異常析出は見られなかった。
図２に示す比較例１の拡大写真（５０００倍）には微細なピンホールが見え、図３に示す比較例２の拡大写真（５０００倍）に大きなピンホールが見える。また、図４に示す比較例３の拡大写真（５００倍）にＮｉ高さの減少及びＰ／Ｎ極の電位差の影響が観察される。特にＮ極にはＮｉが析出しにくい。更に図５に示す比較例４の拡大写真（５００倍）で電極パッド部周辺部にＮｉの異常析出（こぶ）が見える。また、図６に示す比較例５の拡大写真（５００倍）にＮｉ高さの減少が、及び拡大写真（５０００倍）に小さいが多数のピンホールが見える。As is clear from FIG. 1, in the example using the electroless Ni plating solution according to the present invention, uniform electroless Ni plating can be performed on the Al pad without being affected by the potential difference and area inherent to the IC. In addition, the Ni deposition rate was sufficient, and Ni pinholes and abnormal precipitation as seen in the comparative examples were not observed.
A fine pinhole is seen in the enlarged photograph (5000 times) of Comparative Example 1 shown in FIG. 2, and a large pinhole is seen in the enlarged photograph (5000 times) of Comparative Example 2 shown in FIG. Moreover, the influence of the reduction | decrease of Ni height and the electric potential difference of a P / N pole is observed by the enlarged photograph (500 times) of the comparative example 3 shown in FIG. In particular, Ni is unlikely to be deposited on the N pole. Further, in the enlarged photograph (500 times) of Comparative Example 4 shown in FIG. 5, abnormal Ni precipitation (kumps) can be seen around the electrode pad portion. In addition, a reduction in Ni height is seen in the enlarged photograph (500 times) of Comparative Example 5 shown in FIG. 6, and a large number of pinholes are visible in the enlarged photograph (5000 times).
本発明に係る無電解Ｎｉめっき液を利用することにより、多数のＩＣチップからなるシリコンウエハー上にも無電解ＮｉめっきによるＮｉ金属バンプ（突起部）もしくははんだバンプ用のＵＢＭを均一な膜厚で形成することが可能なとなる。 By using the electroless Ni plating solution according to the present invention, Ni metal bumps (projections) by electroless Ni plating or UBMs for solder bumps with a uniform film thickness can be formed on a silicon wafer composed of a number of IC chips. It becomes possible to form.
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| PCT/JP2006/319063 WO2007043333A1 (en) | 2005-10-07 | 2006-09-26 | Electroless nickel plating solution |
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| US20120061698A1 (en) * | 2010-09-10 | 2012-03-15 | Toscano Lenora M | Method for Treating Metal Surfaces |
| EP2551375A1 (en) * | 2011-07-26 | 2013-01-30 | Atotech Deutschland GmbH | Electroless nickel plating bath composition |
| US8936672B1 (en) * | 2012-06-22 | 2015-01-20 | Accu-Labs, Inc. | Polishing and electroless nickel compositions, kits, and methods |
| CN103898583A (en) * | 2013-06-03 | 2014-07-02 | 无锡市锡山区鹅湖镇荡口青荡金属制品厂 | Chemical nickel-plating solution electroplating chromium on surface of magnesium alloy die casting |
| JP6163023B2 (en) * | 2013-06-10 | 2017-07-12 | 日本電波工業株式会社 | Quartz device and method of manufacturing quartz device |
| JP6326857B2 (en) * | 2014-02-21 | 2018-05-23 | 三菱瓦斯化学株式会社 | Electroless plating solution |
| US11685999B2 (en) | 2014-06-02 | 2023-06-27 | Macdermid Acumen, Inc. | Aqueous electroless nickel plating bath and method of using the same |
| JP6474860B2 (en) * | 2017-06-28 | 2019-02-27 | 小島化学薬品株式会社 | Electroless nickel strike plating solution and method for forming nickel plating film |
| CN110527992A (en) * | 2019-09-27 | 2019-12-03 | 广州皓悦新材料科技有限公司 | A kind of chemical nickel-plating plating solution |
| KR102121755B1 (en) * | 2020-02-20 | 2020-06-12 | 주식회사 씨엠케미칼 | An electroless nickel plating solution easy to convert use |
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| JP3687722B2 (en) * | 1999-01-12 | 2005-08-24 | 上村工業株式会社 | Electroless composite plating solution and electroless composite plating method |
| JP3499543B2 (en) * | 2001-08-15 | 2004-02-23 | 株式会社神戸製鋼所 | Electrical Zn-plated steel sheet with excellent white rust resistance and method for producing the same |
| CN1150349C (en) * | 2001-09-29 | 2004-05-19 | 中国科学院金属研究所 | Method of supersonic chemical plating nickel phosphorus of powder metallurgy material |
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2006
- 2006-09-26 WO PCT/JP2006/319063 patent/WO2007043333A1/en active Application Filing
- 2006-09-26 KR KR1020077030494A patent/KR100961011B1/en not_active IP Right Cessation
- 2006-09-26 US US11/920,021 patent/US8182594B2/en not_active Expired - Fee Related
- 2006-09-26 JP JP2007539858A patent/JP4536781B2/en not_active Expired - Fee Related
- 2006-09-26 EP EP06798329.6A patent/EP1932943A4/en not_active Withdrawn
- 2006-09-26 CN CN2006800193775A patent/CN101189362B/en not_active Expired - Fee Related
- 2006-10-03 TW TW095136656A patent/TWI337628B/en not_active IP Right Cessation
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS533326B1 (en) * | 1971-07-06 | 1978-02-06 | ||
| JPH06280038A (en) * | 1993-03-30 | 1994-10-04 | Hitachi Chem Co Ltd | Electroless nickel-phosphorus plating solution |
| JPH07233479A (en) * | 1994-02-21 | 1995-09-05 | Tetsuya Aisaka | Electroless plating bath and electroless plating method |
| JPH09176864A (en) * | 1995-10-23 | 1997-07-08 | C Uyemura & Co Ltd | Thick-film formation in electroless gold plating |
| JP2003268561A (en) * | 2002-03-15 | 2003-09-25 | Murata Mfg Co Ltd | Electroless plating solution, method of producing ceramic electronic parts, and ceramic electronic parts |
Also Published As
| Publication number | Publication date |
|---|---|
| US8182594B2 (en) | 2012-05-22 |
| EP1932943A1 (en) | 2008-06-18 |
| CN101189362B (en) | 2011-03-16 |
| JPWO2007043333A1 (en) | 2009-04-16 |
| TW200720477A (en) | 2007-06-01 |
| TWI337628B (en) | 2011-02-21 |
| EP1932943A4 (en) | 2013-06-26 |
| US20090064892A1 (en) | 2009-03-12 |
| KR20080015463A (en) | 2008-02-19 |
| KR100961011B1 (en) | 2010-06-01 |
| CN101189362A (en) | 2008-05-28 |
| WO2007043333A1 (en) | 2007-04-19 |
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